data_alf2__xx1 _audit_creation_method SHELXL-97 _chemical_name_common 'oxy hydroxy bismuth sulphate' _chemical_name_mineral 'cannonite' _chemical_formula_sum 'Bi2 H2 O7 S' _chemical_formula_weight 564.04 _chemical_compound_source 'Alfenza Mine, Crodo, Italy' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7196(5) _cell_length_b 13.8856(9) _cell_length_c 5.6980(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.1740(10) _cell_angle_gamma 90.00 _cell_volume 576.89(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1222 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 6.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 61.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.066 _exptl_absorpt_correction_T_max 0.294 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD' _diffrn_measurement_method '\w' _diffrn_reflns_number 6856 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1320 _reflns_number_gt 1222 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker AXS)' _computing_cell_refinement 'SMART (Bruker AXS)' _computing_data_reduction 'SAINT (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker (CrystalMaker software, ltd)' _computing_publication_material 'WinGX, Ferrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1320 _refine_ls_number_parameters 100 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.53592(6) 0.15668(3) 0.40485(7) 0.0139(2) Uani 0.957(10) 1 d P . . Bi2 Bi 0.19011(7) 0.13417(4) 0.71336(9) 0.0175(2) Uani 0.947(9) 1 d P . . S1 S 0.8750(4) 0.1333(2) 0.0967(5) 0.0142(8) Uani 1 1 d . . . O5 O 0.3890(11) 0.2318(6) 0.6467(14) 0.0189(19) Uani 1 1 d . . . OH1 O 0.3234(12) 0.0524(6) 0.4989(15) 0.0215(19) Uani 1 1 d D . . H1 H 0.218(7) 0.021(7) 0.376(17) 0.032 Uiso 1 1 d D . . OH2 O 0.3967(12) 0.0741(6) 0.0349(15) 0.0216(19) Uani 1 1 d D . . H2 H 0.297(11) 0.029(7) 0.04(2) 0.032 Uiso 1 1 d D . . O1A O 0.7396(13) 0.2025(7) 0.1265(16) 0.030(2) Uani 1 1 d . . . O2A O 0.9028(14) 0.0587(6) 0.2936(16) 0.029(2) Uani 1 1 d . . . O3 O 0.0511(13) 0.1822(8) 0.139(2) 0.036(3) Uani 1 1 d . . . O4 O 0.8095(14) 0.0891(7) -0.1505(16) 0.032(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.0101(3) 0.0177(3) 0.0105(3) 0.00068(13) -0.0011(2) 0.00039(15) Bi2 0.0111(3) 0.0215(3) 0.0184(3) 0.00136(16) 0.0028(2) 0.00032(18) S1 0.0075(15) 0.0191(14) 0.0120(13) -0.0003(10) -0.0022(10) -0.0016(11) O5 0.016(5) 0.022(4) 0.019(4) -0.006(3) 0.005(3) -0.006(3) OH1 0.018(5) 0.024(4) 0.021(4) -0.007(3) 0.005(4) -0.007(4) OH2 0.016(5) 0.024(4) 0.018(4) -0.003(3) -0.003(4) -0.002(4) O1A 0.026(5) 0.037(5) 0.029(5) 0.009(4) 0.010(4) 0.013(4) O2A 0.032(6) 0.027(5) 0.023(4) 0.015(3) 0.004(4) 0.009(4) O3 0.008(5) 0.041(6) 0.057(7) -0.004(5) 0.006(5) -0.014(4) O4 0.035(6) 0.029(5) 0.022(4) -0.008(4) -0.003(4) -0.005(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O5 2.180(8) 4_565 ? Bi1 O5 2.302(7) . ? Bi1 OH2 2.329(8) . ? Bi1 OH1 2.377(8) . ? Bi1 O1A 2.567(9) 4_566 ? Bi1 O1A 2.651(9) . ? Bi1 O4 2.872(9) 1_556 ? Bi1 Bi2 3.6601(6) . ? Bi2 OH1 2.160(8) . ? Bi2 OH2 2.162(8) 1_556 ? Bi2 O5 2.173(8) . ? Bi2 O3 2.745(10) 4_566 ? Bi2 O2A 2.770(9) 3_656 ? Bi2 O2A 2.873(10) 1_455 ? S1 O4 1.466(9) . ? S1 O3 1.467(9) 1_655 ? S1 O1A 1.470(9) . ? S1 O2A 1.490(8) . ? O5 Bi1 2.180(8) 4_566 ? OH1 H1 0.98(2) . ? OH2 Bi2 2.162(8) 1_554 ? OH2 H2 0.99(2) . ? O1A Bi1 2.567(9) 4_565 ? O3 S1 1.467(9) 1_455 ? O3 Bi2 2.745(10) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Bi1 O5 80.37(18) 4_565 . ? O5 Bi1 OH2 75.9(3) 4_565 . ? O5 Bi1 OH2 126.4(3) . . ? O5 Bi1 OH1 109.9(3) 4_565 . ? O5 Bi1 OH1 68.2(3) . . ? OH2 Bi1 OH1 75.9(3) . . ? O5 Bi1 O1A 83.7(3) 4_565 4_566 ? O5 Bi1 O1A 72.7(3) . 4_566 ? OH2 Bi1 O1A 147.8(3) . 4_566 ? OH1 Bi1 O1A 135.2(3) . 4_566 ? O5 Bi1 O1A 72.9(3) 4_565 . ? O5 Bi1 O1A 139.0(3) . . ? OH2 Bi1 O1A 76.4(3) . . ? OH1 Bi1 O1A 150.4(3) . . ? O1A Bi1 O1A 74.0(3) 4_566 . ? O5 Bi1 O4 153.7(3) 4_565 1_556 ? O5 Bi1 O4 89.1(3) . 1_556 ? OH2 Bi1 O4 128.7(3) . 1_556 ? OH1 Bi1 O4 87.9(3) . 1_556 ? O1A Bi1 O4 70.2(3) 4_566 1_556 ? O1A Bi1 O4 101.4(3) . 1_556 ? O5 Bi1 Bi2 94.9(2) 4_565 . ? O5 Bi1 Bi2 33.99(19) . . ? OH2 Bi1 Bi2 101.5(2) . . ? OH1 Bi1 Bi2 34.27(19) . . ? O1A Bi1 Bi2 104.73(19) 4_566 . ? O1A Bi1 Bi2 167.72(19) . . ? O4 Bi1 Bi2 89.4(2) 1_556 . ? OH1 Bi2 OH2 85.5(3) . 1_556 ? OH1 Bi2 O5 74.6(3) . . ? OH2 Bi2 O5 91.3(3) 1_556 . ? OH1 Bi2 O3 129.4(3) . 4_566 ? OH2 Bi2 O3 129.2(3) 1_556 4_566 ? O5 Bi2 O3 69.9(3) . 4_566 ? OH1 Bi2 O2A 69.7(3) . 3_656 ? OH2 Bi2 O2A 75.8(3) 1_556 3_656 ? O5 Bi2 O2A 142.7(3) . 3_656 ? O3 Bi2 O2A 144.1(3) 4_566 3_656 ? OH1 Bi2 O2A 73.7(3) . 1_455 ? OH2 Bi2 O2A 135.9(3) 1_556 1_455 ? O5 Bi2 O2A 118.6(3) . 1_455 ? O3 Bi2 O2A 93.1(3) 4_566 1_455 ? O2A Bi2 O2A 60.7(3) 3_656 1_455 ? OH1 Bi2 Bi1 38.3(2) . . ? OH2 Bi2 Bi1 89.4(2) 1_556 . ? O5 Bi2 Bi1 36.3(2) . . ? O3 Bi2 Bi1 99.0(2) 4_566 . ? O2A Bi2 Bi1 107.58(19) 3_656 . ? O2A Bi2 Bi1 96.70(18) 1_455 . ? O4 S1 O3 111.0(6) . 1_655 ? O4 S1 O1A 110.5(6) . . ? O3 S1 O1A 109.6(6) 1_655 . ? O4 S1 O2A 110.6(6) . . ? O3 S1 O2A 107.6(6) 1_655 . ? O1A S1 O2A 107.4(5) . . ? Bi2 O5 Bi1 124.5(3) . 4_566 ? Bi2 O5 Bi1 109.7(3) . . ? Bi1 O5 Bi1 118.5(3) 4_566 . ? Bi2 OH1 Bi1 107.4(3) . . ? Bi2 OH1 H1 101(4) . . ? Bi1 OH1 H1 125(7) . . ? Bi2 OH2 Bi1 124.7(4) 1_554 . ? Bi2 OH2 H2 84(6) 1_554 . ? Bi1 OH2 H2 115(8) . . ? S1 O1A Bi1 141.7(5) . 4_565 ? S1 O1A Bi1 119.8(5) . . ? Bi1 O1A Bi1 95.1(3) 4_565 . ? S1 O3 Bi2 138.5(6) 1_455 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OH1 H1 O4 0.98(2) 1.97(5) 2.742(12) 134(5) 3_655 OH2 H2 O4 0.99(2) 2.03(4) 2.965(13) 155(9) 3_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.437 _refine_diff_density_min -4.586 _refine_diff_density_rms 0.755 data_alf2_xx2 _audit_creation_method SHELXL-97 _chemical_name_common 'oxy hydroxy bismuth sulphate' _chemical_name_mineral 'cannonite' _chemical_compound_source 'Alfenza Mine, Crodo, Italy' _chemical_formula_sum 'Bi2 H2 O7 S' _chemical_formula_weight 564.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7100(8) _cell_length_b 13.8717(14) _cell_length_c 5.6939(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.155(2) _cell_angle_gamma 90.00 _cell_volume 575.25(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1691 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 31.54 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.015 _exptl_crystal_density_diffrn 6.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 61.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.065 _exptl_absorpt_correction_T_max 0.398 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex CCD' _diffrn_measurement_method '\w' _diffrn_reflns_number 6215 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 31.54 _reflns_number_total 1799 _reflns_number_gt 1691 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker AXS)' _computing_cell_refinement 'SMART (Bruker AXS)' _computing_data_reduction 'SAINT (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker (CrystalMaker software, ltd)' _computing_publication_material 'WinGX, Ferrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+11.2240P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 1799 _refine_ls_number_parameters 99 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.53571(5) 0.15677(3) 0.40495(7) 0.01278(15) Uani 0.993(11) 1 d P . . Bi2 Bi 0.18996(6) 0.13408(3) 0.71332(8) 0.01638(16) Uani 0.981(11) 1 d P . . S1 S 0.8755(4) 0.13304(18) 0.0977(5) 0.0114(6) Uani 1 1 d . . . O5 O 0.3891(11) 0.2322(6) 0.6478(15) 0.0170(16) Uani 1 1 d . . . OH1 O 0.3277(11) 0.0527(6) 0.5021(15) 0.0175(16) Uani 1 1 d D . . H1 H 0.235(13) 0.028(6) 0.353(17) 0.026 Uiso 1 1 d D . . OH2 O 0.3953(13) 0.0746(6) 0.0381(15) 0.0197(17) Uani 1 1 d D . . H2 H 0.34(2) 0.012(5) 0.06(3) 0.030 Uiso 1 1 d D . . O1A O 0.7384(13) 0.2038(7) 0.1278(17) 0.0248(19) Uani 1 1 d . . . O2A O 0.9019(14) 0.0594(7) 0.2913(16) 0.026(2) Uani 1 1 d . . . O3 O 0.0480(14) 0.1832(8) 0.136(2) 0.033(2) Uani 1 1 d . . . O4 O 0.8083(18) 0.0891(7) -0.1490(16) 0.035(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.0070(2) 0.0157(2) 0.0149(2) 0.00072(11) 0.00259(15) 0.00058(11) Bi2 0.0076(2) 0.0195(3) 0.0231(3) 0.00124(14) 0.00650(17) 0.00031(13) S1 0.0062(11) 0.0137(11) 0.0142(11) -0.0023(8) 0.0031(8) -0.0022(8) O5 0.011(3) 0.014(4) 0.025(4) -0.003(3) 0.005(3) -0.002(3) OH1 0.012(3) 0.019(4) 0.022(4) -0.008(3) 0.006(3) -0.004(3) OH2 0.021(4) 0.022(4) 0.014(3) 0.000(3) 0.003(3) -0.003(3) O1A 0.021(4) 0.027(4) 0.030(4) 0.009(3) 0.014(4) 0.011(3) O2A 0.025(5) 0.029(5) 0.019(4) 0.017(3) 0.002(3) 0.003(4) O3 0.014(4) 0.029(5) 0.052(6) -0.001(4) 0.006(4) -0.011(4) O4 0.062(8) 0.022(4) 0.011(4) 0.000(3) 0.000(4) -0.002(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 O5 2.170(8) 4_565 ? Bi1 O5 2.304(8) . ? Bi1 OH2 2.313(8) . ? Bi1 OH1 2.355(8) . ? Bi1 O1A 2.548(9) 4_566 ? Bi1 O1A 2.641(9) . ? Bi1 O4 2.872(10) 1_556 ? Bi1 Bi2 3.6551(6) . ? Bi2 OH1 2.164(8) . ? Bi2 OH2 2.165(8) 1_556 ? Bi2 O5 2.173(8) . ? Bi2 O3 2.739(10) 4_566 ? Bi2 O2A 2.774(10) 3_656 ? Bi2 O2A 2.877(10) 1_455 ? S1 O3 1.453(10) 1_655 ? S1 O4 1.461(9) . ? S1 O2A 1.467(8) . ? S1 O1A 1.493(9) . ? O5 Bi1 2.170(8) 4_566 ? OH1 H1 0.98(2) . ? OH2 Bi2 2.165(8) 1_554 ? OH2 H2 0.98(2) . ? O1A Bi1 2.548(9) 4_565 ? O3 S1 1.453(10) 1_455 ? O3 Bi2 2.739(10) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Bi1 O5 80.39(19) 4_565 . ? O5 Bi1 OH2 75.8(3) 4_565 . ? O5 Bi1 OH2 126.1(3) . . ? O5 Bi1 OH1 110.5(3) 4_565 . ? O5 Bi1 OH1 68.3(3) . . ? OH2 Bi1 OH1 75.9(3) . . ? O5 Bi1 O1A 84.0(3) 4_565 4_566 ? O5 Bi1 O1A 72.4(3) . 4_566 ? OH2 Bi1 O1A 148.5(3) . 4_566 ? OH1 Bi1 O1A 134.6(3) . 4_566 ? O5 Bi1 O1A 72.6(3) 4_565 . ? O5 Bi1 O1A 138.5(3) . . ? OH2 Bi1 O1A 77.0(3) . . ? OH1 Bi1 O1A 150.9(3) . . ? O1A Bi1 O1A 74.0(3) 4_566 . ? O5 Bi1 O4 153.8(3) 4_565 1_556 ? O5 Bi1 O4 88.8(3) . 1_556 ? OH2 Bi1 O4 128.8(3) . 1_556 ? OH1 Bi1 O4 87.1(3) . 1_556 ? O1A Bi1 O4 69.9(3) 4_566 1_556 ? O1A Bi1 O4 101.8(3) . 1_556 ? O5 Bi1 Bi2 94.9(2) 4_565 . ? O5 Bi1 Bi2 34.1(2) . . ? OH2 Bi1 Bi2 101.1(2) . . ? OH1 Bi1 Bi2 34.30(19) . . ? O1A Bi1 Bi2 104.5(2) 4_566 . ? O1A Bi1 Bi2 167.43(19) . . ? O4 Bi1 Bi2 89.1(2) 1_556 . ? OH1 Bi2 OH2 85.5(3) . 1_556 ? OH1 Bi2 O5 74.2(3) . . ? OH2 Bi2 O5 91.5(3) 1_556 . ? OH1 Bi2 O3 129.5(3) . 4_566 ? OH2 Bi2 O3 129.2(3) 1_556 4_566 ? O5 Bi2 O3 70.1(3) . 4_566 ? OH1 Bi2 O2A 70.2(3) . 3_656 ? OH2 Bi2 O2A 75.6(3) 1_556 3_656 ? O5 Bi2 O2A 142.8(3) . 3_656 ? O3 Bi2 O2A 143.8(3) 4_566 3_656 ? OH1 Bi2 O2A 74.5(3) . 1_455 ? OH2 Bi2 O2A 136.4(3) 1_556 1_455 ? O5 Bi2 O2A 118.5(3) . 1_455 ? O3 Bi2 O2A 92.3(3) 4_566 1_455 ? O2A Bi2 O2A 61.2(3) 3_656 1_455 ? OH1 Bi2 Bi1 37.8(2) . . ? OH2 Bi2 Bi1 89.9(2) 1_556 . ? O5 Bi2 Bi1 36.5(2) . . ? O3 Bi2 Bi1 99.1(2) 4_566 . ? O2A Bi2 Bi1 107.6(2) 3_656 . ? O2A Bi2 Bi1 96.57(19) 1_455 . ? O3 S1 O4 111.2(7) 1_655 . ? O3 S1 O2A 109.1(6) 1_655 . ? O4 S1 O2A 110.5(6) . . ? O3 S1 O1A 108.4(6) 1_655 . ? O4 S1 O1A 110.1(6) . . ? O2A S1 O1A 107.5(5) . . ? Bi1 O5 Bi2 124.7(4) 4_566 . ? Bi1 O5 Bi1 118.5(4) 4_566 . ? Bi2 O5 Bi1 109.4(3) . . ? Bi2 OH1 Bi1 107.9(3) . . ? Bi2 OH1 H1 108(7) . . ? Bi1 OH1 H1 112(9) . . ? Bi2 OH2 Bi1 125.3(4) 1_554 . ? Bi2 OH2 H2 102(10) 1_554 . ? Bi1 OH2 H2 115(9) . . ? S1 O1A Bi1 141.6(5) . 4_565 ? S1 O1A Bi1 119.1(5) . . ? Bi1 O1A Bi1 95.7(3) 4_565 . ? S1 O3 Bi2 139.9(7) 1_455 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OH1 H1 O4 0.98(2) 1.96(5) 2.762(12) 138(6) 3_655 OH2 H2 O4 0.98(2) 2.00(4) 2.944(14) 162(11) 3_655 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 31.54 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 6.723 _refine_diff_density_min -5.543 _refine_diff_density_rms 0.721